DE1544761A1 - Process for the production of polyvinyl chloride suitable for age-resistant plastisols - Google Patents

Description

Process for the production of non-aging plastisols suitable polyvinyl chloride

It is "known from polyvinyl chloride, which is produced by the emulsion process was made to prepare more or less viscous pastes, by comminuting the product to specific grain sizes and mixing it with plasticizers. The flow properties of these The masses depend essentially on the particle size distribution of the polyvinyl chloride and on the type of plasticizer. Most Polyvinyl chloride types found on the Harkt, for so-called Plastisols are suitable have the disadvantage that they as pastes because the polyvinyl chloride can also age at normal room temperature is plasticizer-soluble, so that an increase in viscosity can be determined after a short standing time · each According to the processing method, they become low or high viscose i'ypes needed. This was achieved, for example, by adding alkali salts polyacrylic acid, the viscosity of plastisol ” increase without affecting the flow behavior. Conversely, you can add polyvinyl chloride with a coarser grain size distribution lower the viscosity. The desired setting of the viscosity in connection with the desired flow behavior (pseudoplastic, thixotropic, Newtonian, dilatant or rheopect, see Rubber and Plastics Age, Febr. 1961 »pages 183-186) is hardly possible from a given type of polyvinyl chloride, even with various plasticizers and additives Yersxiohö, through other additives such as polymer solutions or others Polyvinyl chloride types to obtain the desired setting, are time consuming and not always reproducible.

Most types of paste polyvinyl chloride also have larger sizes Particles and with them the disadvantage that they result in speckled plaat sols. These lead particularly in the production of thin films to irregular surfaces and poor mechanical properties

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Values of the plasticized material _o Furthermore, sxe have the disadvantage that "if the calibration is high, the plastisol © tend to sediment". The aging resistance is thereby considerably reduced.

The present invention is now a process for preparing suitable for aging-resistant plastisols of polyvinyl chloride, which is characterized in that ge _ö en mechanical stress, weak illektrolyte and sedimentation stable polyvinyl chloride dispersions fatty acids having 8 to 22 carbon atoms, preferably 10 to 18 carbon atoms, or their ammonium or aliphatic amine salts or the corresponding fatty alcohols, or mixtures of such substances are emulsified in an amount of 0.1 to 5 %, preferably 0.5 to 2%, the resulting emulsions with atomization dries and the product is ground. It is expedient to work in such a way that the emulsions are heated to a higher temperature, if necessary up to 90 ° C., for up to 60 minutes, preferably 5 to 15 minutes, before spray drying.

It has been found that by adding fatty alcohols to a fully polymerized polyvinyl chloride latex and subsequent processing in an atomization dryer one over several Days aging-resistant paste with the addition of phthalate softeners to. is obtained, which is low depending on the amount of fatty alcohol added

viscos and a pseudoplastic flow - in extreme cases an ointment-like state - shows. This flow behavior is particularly desirable if you want to coat fabric on one side with this paste or if you work according to the dip process. The Al, Chipping resistance of these "ointments" may be increased if the latex is brought 60 80 ⁰ C before its processing, but under .Zusatz of fatty alcohols for a short time at an elevated temperature, for example. Even better results can be achieved if a water-soluble fatty acid salt of ammonium or of alkylamines - which are also to be understood as alkylolamines - is added to the latex described above. This makes the polyvinyl chloride even less soluble in the paste and thus more stable in terms of viscosity at room temperature or at a slightly elevated temperature. Only above a certain temperature

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- about 80-C - the quick, desired gelatinization then occurs. On the other hand, thin, weakly thixotropic, almost non-toxic plastisols are obtained if free fatty acids are added to the starting emulsion and then worked up by spray drying Mix the usual plasticizers up to a solids content of 70 rfo to form more or less viscous pastes, depending on the solids content, which are free of specks and resistant to aging Days). These pastes are particularly suitable for the spin or rotation ^ ußverfahren and enter the gelation very smooth and flat Oberflächeno The flow properties described require relatively low starting temperatures for atomization, 'ie, "if possible under 70 C ^-," Till you dilatant to rheopecte pastes to 85 C, atomised - obtained, so a higher starting temperature, zS ₀ at 80 under the same must Zusätzen'bei.

Example 1;

A polyvinyl chloride latex with a solids content of 48 f ° f with the addition of Hersolat K JO, (trade name) phosphate buffer and hydrogen peroxide was prepared according to a conventional polymerization process and shows high mechanical stability, was emulsified with emulsification of '1' fo fatty acid mixture, a so-called. Eokosoel fatty acid blend of Cj ₀ - Cj _fi ~ acid added, heated to 80 G for 10 minutes and then at a dry air outlet temperature between 55 and 65 C (measured at the Irennstelie of moist air and polyvinyl chloride) by spray drying worked up. The product can be at high speed from the Stiftnühlen i'yp Colloplex a 'feilchengrÖße of 2 my smaller and deagglomerate, liach admixture with 40 "/ ο Diox-frylphthalat obtained a storage stable, speck. free plastisol that can be processed without homogenizing machines. The viscosity of this 60 $ polyvinyl chloride paste is only 4,000 cP (measured in the Brookfield Tiscosimeter Rl ¹ S ¹ J with spindle 6 at 100 TJpM "^ 20 ⁰ C)", after 15 days or "30 days

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Life at room temperature was unchanged _β the Yiscosität

Example 2; '

v / ie example 1, but without heating the lümulsion. You get under the conditions described above, a plastisol that shows ps eudoplastic flow, initial viscosity of 4000 cP, which after 10 days of standing to 8000 cP has risen »

Example 5 * - ■

Sine emulsion is the addition of 1 fi 3? Ettsäureamiaonsalz (C ^ / Cq acid) was added and 10 I.Iinuten to 60 C heated "After the work-up and mix with 50 ° / ° Tieichmacher obtained a highly thixotropic chamfered whose From £ angular viscosity at rpm = 2,000 cP. A viacosity of 20,000 cPo is measured with one rotation

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Claims (1)

'ra ** Patent claims: ο A process for the production of polyvinyl chloride suitable for aging-resistant plastisols, characterized in that polyvinyl chloride dispersions, which are stable to mechanical stress, weak electrolytes and sedimentation, are fatty acids with 8 to 22 carbon atoms, or preferably 10 to 18 G atoms, b ^ w. their Aumon or aliphatic amine salts or the corresponding ij'ett alcohols, or mixtures of such substances in an amount of 0.1 to 5 ×, preferably 0.5 to 2 γ, _ emulsified into the resulting emulsions with atomization dries and the product wilts. . J- 2ο The method according to claim 1, characterized in that one the .emulsions before spray drying up to bO lu minutes, preferably 5 to 15 minutes, to a higher one 'i' temperature, if necessary up to 90 G, erv / ärmto Dr.Iii / Häo 9098 16/0679 _BAD original